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US8772014B2 - Method for stabilization of biological cultures to allow biological treatment of brines - Google Patents

Method for stabilization of biological cultures to allow biological treatment of brines Download PDF

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US8772014B2
US8772014B2 US10/579,640 US57964004A US8772014B2 US 8772014 B2 US8772014 B2 US 8772014B2 US 57964004 A US57964004 A US 57964004A US 8772014 B2 US8772014 B2 US 8772014B2
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pollutant
brine solution
ion
perchlorate
divalent
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US20070275450A1 (en
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Deborah J. Roberts
Dennis A. Clifford
Xiaohua Lin
Thomas Gillogly
Lee Aldridge
Stewart Lehman
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University of Houston System
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University of Houston System
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/28—Anaerobic digestion processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/16—Nitrogen compounds, e.g. ammonia
    • C02F2101/163—Nitrates
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/08—Seawater, e.g. for desalination
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel

Definitions

  • This invention was made in part with government support under Account #2805 awarded by the MWH/AWWARF. This invention was also made in part from the University of Houston under the grant number 1551320 (cost Center #00730-5022-H0068-B0001-G086414.
  • the present invention relates to a composition for stabilizing biological cultures in brine solutions under anaerobic/anoxic conditions and to a process for treating brine solutions biologically under anaerobic/anoxic conditions, where the cultures include one or a plurality of microorganisms capable degrading a desired pollutant in a brine solution.
  • the present invention relates to a composition for stabilizing a biological culture in a brine solution under anaerobic/anoxic conditions, where the composition includes an effective amount of a divalent cation, where the effective amount of the divalent cation is sufficient to produce a divalent/monovalent cation ratio in the brine solution of at least a 0.05 mole/mole or a divalent/monovalent cation ratio greater than or equal to 0.05 mole/mole, where the ratio promotes growth and sustained proliferation of biological microorganisms capable of degrading pollutants or decreasing a concentration of pollutants in the brine solution.
  • the present invention relates to a method using the composition to treat contaminated brine solutions under anaerobic/anoxic conditions.
  • the stabilized brine solutions are geared to stably grow perchlorate degrading microorganism. In another preferred embodiment, the stabilized brine solutions are geared to stably grow perchlorate and nitrate degrading microorganisms.
  • wastes stream are composed of aqueous salt solutions such as ion-exchange brines, oilfield production brines, spent caustic solution, and brines produced during chemical processes that contain elevated levels or concentrations of salts such as Na + .
  • aqueous salt solutions such as ion-exchange brines, oilfield production brines, spent caustic solution, and brines produced during chemical processes that contain elevated levels or concentrations of salts such as Na + .
  • These waste stream may also contain contaminants that would be amenable to biological treatment, microbial treatment, if organisms or microbes could function in high salt waste streams.
  • a method for the treatment of wastewater, suspected of being contaminated with perchlorates, nitrates, hydrolysates and other energetic materials comprises (a) providing at least one microaerobic reactor containing a mixed bacterial culture capable of reducing perchlorate, nitrate, hydrolysates and other energetic products; (b) feeding contaminated wastewater into the microaerobic reactor; (c) maintaining a microaerobic environment in the microaerobic reactor by at least one method selected from the group consisting of (i) mixing air and nitrogen gas and sparging or purging the reactor with the gas mixture; (ii) using a nitrogen membrane separator to provide a low oxygen-containing nitrogen gas to the reactor for sparging or purging; (iii) adding air to the reactor for sparging or purging as necessary to maintain a target dissolved oxygen concentration or a target oxygen concentration in head space gas present in the reactor; and (iv) adding and/or maintaining oxygenated ions
  • Microbial perchlorate reduction under anaerobic conditions has been studied by many researchers. See for example Attaway and Smith, 1993; Herman and Frankenberger, 1999; Logan et al., 2001a; Rikken et al., 1996. Many microorganisms can reduce perchlorate to harmless chloride. Unfortunately, most known perchlorate-reducing microorganisms cannot endure high salinity in the growth media, and usually require less than 2% to 3% NaCl. See for example Coates et al. (2000), Malmqvist et al. (1994), and Michaelidou et al. (2000).
  • the present invention provides a composition including a brine solution including a pollutant, where the brine solution has an effective divalent to monovalent cation mole ratio and where the effective ratio is sufficient to promote stable microbial proliferation in a brine solution under anaerobic/anoxic conditions, where the microbes are capable of degrading the pollutant under anaerobic/anoxic conditions.
  • Preferred cultures are cultures that are capable of degrading perchlorate and/or nitrate in stabilized brine solutions of this invention.
  • the present invention also provides a brine solution including a pollutant and an effective amount of a divalent ratio, where the effective amount is sufficient to adjust a divalent to monovalent cation mole ratio into a range capable of supporting stable microorganism growth and proliferation under anaerobic/anoxic conditions, where the microorganism or microorganisms are capable of reducing a concentration of the pollutant in the brine solution to a desired level, preferably a level below a set governmental standard or below a detection limit for a governmentally accepted analytical technique.
  • perchlorates, nitrates, hydrolysates and other energetics can be reduced to a desired low level and preferably below non-detectable concentrations, in a safe and cost effective manner, using readily available non-toxic low cost nutrients.
  • the treatment of this invention results in the degradation of a significantly higher concentrations of perchlorate, nitrate, etc. ( ⁇ 1.5 wt %) than was previously possible, especially in brine solution having a salinity greater than 3%.
  • the salinity ranges from about 3% to about 18%.
  • the salinity ranges from about 3% to about 15%.
  • the salinity ranges from about 3% to about 12%.
  • the salinity ranges from about 3% to about 10%.
  • the present invention also provides a brine solution including a pollutant and having an effective divalent to monovalent cation ratio, where the effective ratio is sufficient to stabilize a biological treatment system including at least one microorganism, where the at least one microorganism is capable ofreducing a concentration of the pollutant in the brine solution under anaerobic/anoxic conditions, degrading the pollutant in the brine solution or eliminating the pollutant in the brine solution and where a rate of pollutant reduction is similar to (within ⁇ 10%) of a rate of pollutant reduction of an equivalently polluted freshwater solution.
  • the present invention provides a method including the step of adding an effective amount of a soluble divalent metal complex to a brine solution to form an biologically compatible brine solution, where the effective amount of the complex is sufficient to adjust a divalent to monovalent cation mole ratio to a numeric value greater than or equal to about 0.05 and where the biologically compatible brine solution is capable of supporting and sustaining microbes or microorganisms having pollutant reduction or degradation properties under anaerobic/anoxic conditions.
  • the present invention provides a method including the steps of analyzing a brine solution to determine a divalent to monovalent cation mole ratio and adding an effective amount of a soluble divalent metal complex to the brine solution, where the effective amount of the soluble divalent metal complex is sufficient to form an biologically compatible brine solution, where the effective amount of the complex is sufficient to adjust a divalent to monovalent cation mole ratio to a numeric value greater than or equal to about 0.05 and where the biologically compatible brine solution is capable of supporting and sustaining microbes or microorganisms having pollutant reduction or degradation properties under anaerobic/anoxic conditions.
  • perchlorates, nitrates, hydrolysates and other energetics can be reduced to non-detectable concentrations, in a safe and cost effective manner, using readily available non-toxic low cost nutrients.
  • the method can also be used to degrade other brine solution pollutants by a judicious choice of microbes capable of degrading a given pollutant.
  • brine solution means any aqueous solution having dissolved therein a sufficient amount of a monovalent alkali metal salt to have a salinity of 3% or more.
  • microbe means a microorganism capable of degrading a particular pollutant in a stabilized brine solution of this invention, where the exact microorganism will depend on the pollutant to be degraded.
  • microorganism means a one celled or multi-celled living organism capable of degrading a particular pollutant in a stabilized brine solution of this invention, where the exact microorganism will depend on the pollutant to be degraded.
  • Under anaerobic/anoxic conditions mean conditions in which no oxygen or substantially no oxygen is present, by substantially, we mean less than about 500 ppm. As it relates to brine solutions, under anaerobic/anoxic conditions means that the brine solution has no or minimal amount of dissovled oxygen in the solution during the microbial treating step.
  • FIG. 1 depicts a simple schematic of a preferred apparatus of this invention for combined ion-exchange and biological treatment
  • FIG. 2 depicts a plot of data verifying that a biological culture does not degrade perchlorate in the absence of Ca 2+ , Mg 2+ , or K + ions in synthetic brine solution containing 60 g/L NaCl;
  • FIG. 3 depicts a plot of data showing that when Mg 2+ is added to an ion-exchange brine solution at different concentrations, the ability for a biological culture to degrade perchlorate rapidly increases with increasing Mg 2+ concentration;
  • FIG. 4 depicts a plot of data showing that when a culture of perchlorate and nitrate reducing organisms were grown in a synthetic medium containing 60 g/L NaCl and 1100 g/L Mg 2+ a ratio of 0.05 mole Mg 2+ /mole Na + , perchlorate was degraded to non-detectable levels in 2-8 days, whereas the degradation time was less than one day when the Mg 2+ /Na + ratio was increased to 0.1 mole/mole;
  • FIG. 5 depicts a plot of data showing normalized perchlorate degradation rate demonstrating the effect of Magnesium addition on the degradation of perchlorate from ion-exchange brine
  • FIG. 6 depicts a plot of data demonstrating the effect of magnesium ion concentration on the degradation of perchlorate in an ion-exchange brine.
  • composition and method to stabilize biological treatment systems in high saline solution or brine solutions having a high salinity can be constructed where the composition and method permit the sustained growth of microorganisms or microbes capable of reducing pollutant levels in brine solutions under anaerobic/anoxic conditions.
  • the inventors have found that the composition and method are ideally suited for reducing perchlorate ion concentration in ion-exchange brine solutions, again under anaerobic/anoxic conditions.
  • microorganisms are capable of growing that degrade pollutants as rapidly and as stably as if the microorganisms were being grown in an equivalently polluted freshwater solution.
  • a divalent cation such as Mg 2+ or Ca 2+
  • the present invention relates broadly to a brine solution capable of supporting microbial growth under anaerobic/anoxic conditions, where the brine solution has a divalent to monovalent cation mole ratio greater then or equal to 0.05, preferably greater than or equal to 0.1.
  • One preferred embodiment includes a NaCl brine solution having added thereto a sufficient amount of a divalent metal ion, M 2+ ion, to attain the desired molar ratio.
  • the divalent to monovalent cation mole ratio is adjusted by adding between about 100 mg/L M 2+ ions and about 4000 mg/L M 2+ ions, preferably, between about 500 mg/L M 2+ ions and about 3000 mg/L M 2+ ions, particularly, between about 750 mg/L M 2+ ions and about 2000 mg/L M 2+ ions, and an optimal level between about 1000 mg/L M 2+ ions and about 2000 mg/L M 2+ ions to the solution.
  • the exact amount of divalent ion to add depends on the initial ratio of the brine solution.
  • the M 2+ ion is selected from the group consisting of Mg 2+ , Ca 2+ , Sr 2+ and mixtures or combinations thereof, where Mg 2+ is preferred for use in perchlorate contaminated brine solution having high carbonate concentration or in which carbonates are formed.
  • the M 2+ ion is selected from the group consisting of Mg 2+ , Ca 2+ , Sr 2+ , Ba 2+ , and mixtures or combinations thereof.
  • the present invention relates broadly to a method for biologically treating a pollutant contaminated brine solution including the steps of adding an effective amount of a divalent ion source to a brine solution, where the effective amount is sufficient to produce a biologically compatible brine solution capable of supporting and sustaining microbial growth or a biologically stable brine solution.
  • a biologically effective amount of a microbial population can be introduced into the solution under anaerobic/anoxic conditions, where the biologically effective amount of the microbial population is sufficient to improve a reduction of pollutant concentrations in the brine solution compared to brine solution in the absence the effective amount of a divalent cation source.
  • the pollutant degradation propensity of the microbials are similar to the pollutant degradation propensity of the microbials in fresh water.
  • the present invention relates broadly to a method including the steps of passing a waste water stream through an ion-exchange resin column including an ion-exchange resin capable of extracting perchlorate and/or nitrate ions. After the ion-exchange resin fully loaded with perchlorate an/or nitrate ions or after a sufficient extraction time, the flow of the waste water stream is stopped and a stabilized brine solution of this invention having a divalent to monovalent cation mole ratio of at least 0.05 is passed through the ion-exchange resin to produce a contaminated brine solution, where the stabilized brine solution is capable of supporting and sustaining microbial growth.
  • a pollutant degrading effective amount of a microbial composition including one microorganism or a plurality of microorganisms each capable of degrading the perchlorate and/or nitrate ions in the stabilized brine solution to form a microbially active brine solution.
  • the microbially active brine solution is agitated under anaerobic/anoxic conditions for at a temperature and for a time sufficient to degrade the perchlorate and/or nitrate concentrations below a desired concentration.
  • the microbially active brine solution is filtered to remove the microbial composition.
  • a makeup amount of NaCl is added to the stabilized brine solution where the additional NaCl is sufficient to adjust the salinity of the stabilized brine solution.
  • an additional amount of the divalent ion source can be added to the filtered stabilized brine solution, where the amount of additional divalent ion source is sufficient to maintain the ratio of at least 0.05.
  • the stabilized brine solution can then be reused in the perchlorate extraction process.
  • the present method can be adapted for use in treating any type of pollutant contaminated brine solution using a stabilized brine solution of this invention.
  • the present invention operates in the absence of oxygen, i.e., under anaerobic/anoxic conditions, is based on adjusting the divalent to monovalent cation mole ratio of the brine solutions to promote microbial growth and proliferation and requires only the addition of acetate as a nutrient so that the degrading brine solutions of this invention are simpler, easier to maintain and more stable the prior art brine solutions used to degrade pollutants.
  • Suitable divalent ion source for use in this invention includes, without limitation, any soluble divalent metal salt, where the counterion does not adversely after the culture.
  • exemplary examples of the divalent metal salts include, without limitation, divalent metal chlorides, divalent metal bromides, or mixtures or combinations thereof.
  • the preferred salts are chloride salts.
  • suitable divalent ion for use in this invention include, without limitation, magnesium, calcium, strontium, other similar divalent metal cations capable of promoting microbial growth in brine solutions or mixtures or combinations thereof.
  • Suitable microbials or microorganisms for use in this invention include, without limitation, bacteria from capable of growing in the stabilized brine solutions of this invention and capable of degrading the pollutant of interest.
  • suitable pollutants which can be degraded using the compositions and methods of this invention include, without limitation, inorganic pollutants, organic pollutants, or mixtures or combinations thereof.
  • exemplary inorganic pollutants include, without limitation, perchlorates, nitrates, nitrites, or mixture or combinations thereof.
  • exemplary organic pollutants include, without limitation, phenols, PCBs, chlorinated solvents, solvents, sewage, industrial wastes, oils, sludge, other chemical pollutants or mixtures or combination thereof.
  • Suitable solid medium for supporting microbial growth include, without limitation, diatomaceous earth, activated carbon, sand, ion-exchange resin, or mixtures or combinations thereof.
  • Suitable reactors for use in the treating step of this invention include, without limitation, a plug flow, dispersed plug flow, or continuously stirred tank reactor, or as a packed, expanded, or fluidized bed column.
  • Perchlorate is a contaminant found in groundwater that can be removed by an ion-exchange process using an ion-exchange resin. During the process, the resins are regenerated resulting in the formation of brine solutions contaminated with perchlorate. These brine solutions are largely defined by a concentration of NaCl in the brine solution used to regenerate the resin. Typically, the NaCl concentration ranges from as low as about 30 g/L NaCl (a 3% saline solution or a 0.5 M NaCl solution) to as high as about 90 g/L (a 9% saline solution or a 1.5 M NaCl solution). These brine solutions represent waste streams requiring disposal. Generally, the higher the NaCl concentration of the regenerant brine solution, the smaller a volume of the perchlorate-contaminated brine solution generated. These brine solutions can also contain nitrates.
  • Typical water treated in ion-exchange processes includes about 50 to about 100 ⁇ g/L perchlorate and between about 1 to about 20 mg/L nitrate-N. After treating, a brine solution is produced including between about 2.5 and about 10 mg/L perchlorate and between about 150 and about 500 mg/L nitrate-N.
  • a brine solution is produced including between about 2.5 and about 10 mg/L perchlorate and between about 150 and about 500 mg/L nitrate-N.
  • One preferred method of this invention includes the step of using an ion-exchange resin to remove perchlorate from a polluted water. Once the resin is no longer capable of removing perchlorate, the resin is regenerated using a brine solution to produce a perchlorate contaminated brine solution. To the perchlorated contaminated brine solution is added an effective amount of a divalent cation precursor sufficient to adjust a divalent to monovalent cation mole ratio in the perchlorate contaminated brine solution to a numeric value greater than or equal to about 0.05.
  • a treating effective amount of a biological treating composition is added to the brine solution and the solution is agitated for a time and at a temperature sufficient to reduce the perchlorate and/or nitrate concentration to or below a desired low level.
  • the biological treating composition includes at least one microorganism capable of degrading perchlorate ions to chloride ions.
  • FIG. 1 a block diagram of a preferred embodiment of an apparatus for implementing a method of this invention, generally 100 , is shown to include an ion-exchange column 102 filled an ion-exchange resin 104 and having a contaminated waste water input 106 , a brine solution input 108 , a treated water output 110 and a brine solution output 112 .
  • the waste water input 106 is connected to a source of waste water (not shown).
  • Waste water containing ion-exchangeable contaminants including perchlorate and nitrate ions flows from the source through the waste water input 106 and passes through the ion-exchange column 102 and exchanges its ion contaminants to the resin 104 until the ion-exchange resin 104 is no longer capable of exchanging the contaminant ions or for a set period of time.
  • the waste water input 106 is closed by a valve or other similar shut off device (not shown) and the brine solution input 108 is opened by a valve or other similar shut off device (not shown) is connected to a brine solution treatment reactor 114 .
  • the reactor 114 includes a brine solution input 115 a microbial nutrient input 116 connected to a microbial nutrient input source (not shown).
  • the reactor 114 can also include a microbial input for adding microbes to the reactor 114 to maintain an effective concentration of viable microbes in the reactor 114 .
  • the reactor 114 also includes a crude treated brine solution output 118 connected to a filter tank 120 including a filter 122 , where the microbes in the crude treated brine solution are removed by the filter 122 .
  • the filtered treated brine solution flows out of the filter tank 120 via a filtered, treated brine solution output 124 connected to a brine holding tank 126 .
  • the holding tank 126 includes a make up NaCl input 128 connected to a NaCl source (not shown).
  • the holding tank 126 can also include a divalent cation precursor input connected to a source (not shown). In a batch mode, the process would run waster water through the resin column until the resin was exhausted.
  • the waster water feed would then be shut off and the column regenerated.
  • the resulting brine solution is then treated by microbes to remove the pollutants in the brine.
  • the process would include two or more resin columns. One column used to process the waste water while the other is being regenerated.
  • a brine solution is continuously being treated to remove the ion exchanged contaminants, filtered, stored, adjusted with additional NaCl and divalent cation precursor, and recirculated to the regenerating column.
  • the continuous mode not only is nutrients added to the treating reactor, but microbes are also added to maintain a treating level of microbes in the reactor.
  • the entire process is sealed as much as possible to prevent air and the biological reactor is sparged with nitrogen gas to maintain anoxic/anaerobic conditions.
  • the M 2+ is maintained at the optimal ratio to Na + for the best culture stability in the specific brine solutions by addition to the spent brine storage tank.
  • Makeup sodium chloride is added in the sweet brine storage tank.
  • Alterations to the proposed diagram include the use of continuous culture to replace the batch culture.
  • a media filter immediately follows the biological treatment unit to prevent any organisms that did not settle in the reactor from coming in contact with the resin bed.
  • the inocula contained large amounts of reduced sulfide, which was expected to act as a sulfur source for organism growth.
  • Four media containing the basal ingredients specified above were prepared in 30 g/L NaCl: Medium 4 contained no additions; Medium 5 contained 1 g/L yeast extract; Medium 6 contained 0.685 g/L NaNO 3 ; Medium 7 contained 1 g/L yeast extract plus 0.685 g/L NaNO 3 .
  • Two media containing the basal ingredients plus the following additions were made up at 60 g/L NaCl: Medium 8 contained 1 g/L yeast extract, Medium 9 contained 0.685 g/L NaNO 3 and 1 g/L yeast extract.
  • the screening tests were performed by adding 3 g of each anaerobic marine sediment to 100 mL of each medium in a 125-mL serum bottle. The dissolved oxygen in the medium was not removed, however, the headspace of the serum bottle was purged with nitrogen gas for 3 min.
  • the serum bottles were crimp-sealed with butyl-rubber stoppers and mixed on a rotary shaker and incubated at 3072° C. for at least one month. Perchlorate and nitrate (when present) were measured as described below.
  • a fresh sample of 3% (w/v) of Freeport #1 sediment was added to 1.5 L Medium 6 in a 2-L glass bottle reactor with a gas-collection device.
  • the reactor was incubated at 30 ⁇ 2° C. and shaken at a rate of 150 rpm. After the initial nitrate and perchlorate in the reactor were removed, 100 mg/L perchlorate was spiked into the reactor. Nitrate was not included in subsequent spikes or feeds until a stable perchlorate reducing culture was developed. This spike-feed procedure was continued until a reproducible perchlorate reduction rate was obtained. Then the feed protocol was switched from a spiked batch reactor mode to a sequencing-batch reactor (SBR) mode using a 30% replacement.
  • SBR sequencing-batch reactor
  • Medium 4a 4a was prepared by adding 67 mM Na 2 S.9H 2 O, to Medium 4.
  • Medium 4b was prepared by adding 0.1 mL trace metal solution and 0.1 mL 50 g/L KH 2 PO 4 to Medium 4.
  • Medium 4c was prepared by adding 0.5 mL 67 mM Na 2 S.9H 2 O, 0.1 mL trace metal solution, and 0.1 mL 50 g/L KH 2 PO 4 .
  • the trace metal solution consisted of 10 g ammonium molybdate, 0.1 g zinc sulfate, 0.3 g boric acid, 1.5 g ferrous chloride, 10 g cobalt chloride, 0.03 g magnesium chloride, 0.03 g nickel chloride, and 0.1 g aluminum potassium sulfate per liter of water.
  • a second 1.5-L culture was enriched using Medium 4c by increasing the volume of the 90-mL culture from the nutrient test that had received Medium 4c by addition of fresh medium in 500 mL batches each time perchlorate was reduced to nondetect levels.
  • the culture was maintained by spiking 100 mg/L perchlorate every three days. After every five feeds, 1 g/L sodium acetate.3H 2 O was spiked into the reactor as well. For several spike-feed cycles, samples were taken every two hours to measure the perchlorate concentration in the reactor.
  • nitrate-N On the 8th feed of the second large culture, 500 mg/L nitrate-N was spiked with 100 mg/L perchlorate. Sodium acetate (3 g/L) was added as the electron donor for both perchlorate and nitrate reduction. Samples were again taken every 2 h, and the nitrogen gas produced in the reactor was measured in the gas collector. Both nitrate and perchlorate were spiked into the reactor for another two feeds when the perchlorate and nitrate in the current allotment of feed was reduced.
  • Inocula of 10 mL of the Freeport #1 culture that reduced perchlorate at 60 g/L NaCl in the screening experiments were transferred to serum bottles containing 90 mL of Medium 4c adjusted to 60 g/L NaCl. After all of the perchlorate in the medium was removed, 100 mg/L perchlorate was spiked into the culture again. This feed procedure was continued 5-6 times to allow more cell mass to grow. Then 10 mL of the culture was transferred again to 90 mL fresh medium and spiked several times. Samples were taken to test perchlorate reduction by the culture at 60 g/L NaCl.
  • IonPac AS16 anion analytical column (4 mm ⁇ 250 mm) mm) and an AS16 guard column (4 mm ⁇ 50 mm).
  • a 225-mL sample loop was used to measure perchlorate concentration higher than 1 mg/L.
  • the sample loop was switched to 1000 mL to measure lower perchlorate concentrations.
  • the detection limit for perchlorate was 5 ppb in de-ionized water and 500 ppb in the presence of X8 g/L NaCl concentration.
  • a gradient eluent was delivered in order to separate all peaks: Initially, a flow of 5 mM KOH was maintained for 2 min at a flow rate of 1.0 mL/min.
  • the eluent KOH composition was changed to 10 mM in a linear gradient from 2 min to 14 min with the flow rate unchanged. A linear gradient was then used to change the eluent composition to 55 mM KOH from 14 min to 20 min while the flow rate was increased to 1.5 mL/min at 20 min. These conditions were held constant from 20 to 27 min. All water used was de-ionized, reagent grade with 18 MO cm resistivity.
  • Nitrite was analyzed by absorbance using the method described in Methods of Seawater Analysis [ 26] because it could not be resolved from the chloride peak during IC analysis.
  • the absorbance was measured in 1-cm cuvettes at 540 nm with Lambda 3B UV/VIS spectrophotometer, Perkin-Elmer Corporation.
  • the three cultures developed from activated sludge were fed acetate as the electron donor and (1) nitrate and perchlorate, or (2) perchlorate only, or (3) nitrate only as the added electron acceptors at an initial NaCl concentration of 8 g/L.
  • a 30-day sample of six marine sediments incubated in synthetic media with 30 or 60 g/L NaCl revealed that the organisms in only three of the sediments—Freeport #1, Fourchon #1 sand Fourchon #3—were capable of reducing perchlorate. All 1 six sediments reduced at least 98% of the nitrate in all of the media having nitrate (results not shown).
  • the Freeport #1 sediment was selected as the most consistent inoculum and Medium 4 containing perchlorate and nitrate at 30 g/L NaCl was selected as the growth medium to enrich a larger-scale perchlorate reducing culture.
  • This 1.5-L Freeport ##1 culture experienced a 28-day lag period, but was then able to reduce 510 mg/L perchlorate to 4.93 mg/L within 56 days.
  • Nitrate was reduced within the first week of incubation. Thereafter, along with each spike feed of 100 mg/L perchlorate, the perchlorate reduction rate increased, and an increase of the biomass was observed in the reactor. After 3-4 perchlorate spikes, the culture could remove 90% of perchlorate fed in the medium within 30 h.
  • the original Freeport 1 marine sediment was rich, black, and very anaerobic. To determine if there were abiotic factors present in the mud that enabled the culture to reduce perchlorate rapidly, fresh, autoclaved Freeport marine sediment was added to duplicate transfers of the ineffective large culture to determine if this could return the culture to a rapid perchlorate reduction rate. Adding the autoclaved sediment had a beneficial effect. The culture containing sediment-amended medium had less perchlorate remaining after a five-day incubation period than the controls. This trend was again observed after a second spike of perchlorate into the cultures (not shown).
  • Na 2 S and trace minerals were added to the culture.
  • phosphate as a traditional biological nutrient was also examined.
  • Na2S provides sulfur for microbial growth, scavenges oxygen, and reduces the redox potential in the culture. Lower redox potential is helpful to anaerobic perchlorate reduction.
  • the culture growing in trace metal-, phosphate- and Na2S-amended Medium4c was used to create another 1.5 L culture. After several spike feeds of B100 mg/L perchlorate, this culture was capable of removing 70-100 mg/L perchlorate within 8 h. After r 48 daily
  • the preferred concentration of NaCl in the ion-exchange brine is 60 g/L (6%) or higher.
  • Initial batch screening tests provided a culture that was initially capable of reducing perchlorate in a medium that contained 60 g/L NaCl within 45 days, but lost the capability in the subsequent transfer to fresh medium with 60 g/L NaCl. Once it was learned that the 30 g/L culture required sulfide, trace metals and phosphate, these ingredients were added to revive the culture in the 60 g/L medium.
  • the pathway of perchlorate degradation involves the sequential reduction of perchlorate to chlorate, chlorite, and finally, chloride.
  • the analytical method used allowed the detection and quantification of perchlorate, and chlorate, but not chlorite.
  • the chloride produced from the reduction of perchlorate could not be quantified because of high background of NaCl (3-6%) in the media.
  • chlorate was observed only transiently in early enrichment cultures, but was never observed in mature cultures.
  • the completion of the respiration of perchlorate can be inferred by a change in redox potential indicated by the color change of resazurin due to O 2 produced in the final reaction. This was observed, again, in enrichment cultures, but rarely in the mature cultures. This does not mean that complete metabolism was not achieved but only that the O 2 was removed as fast as it was produced.
  • Two cultures capable of degrading perchlorate and nitrate in high salt solutions were developed from marine inoculum.
  • One culture is capable of reducing up to 100 mg/L perchlorate and 500 mg/L nitrate-N within 5 h in the presence of 30 g/L NaCl.
  • the other is capable of reducing 100 mg/L perchlorate in the presence of60 g/L NaCl within 24 h.
  • the growth conditions to maintain these cultures in a healthy state require the maintenance of strictly anaerobic conditions and the addition of trace metals, Na 2 S and phosphate.
  • the cultures were maintained in six, 1.5-L sealed glass bottle reactors as sequencing batch reactors by weekly settling, decanting 50-60% of the supernatant (spent medium) with fresh synthetic media typically once a week. Between the replacements, perchlorate stock solution (100 g/L) was spiked in the cultures to a final perchlorate concentration of about 100 mg/L, daily. Acetate served as the sole electron donor. Prior to each experiment, volatile suspended solids (VSS) concentration was measured for the Parent culture so that VSS concentration present in the subcultures could be estimated.
  • VSS volatile suspended solids
  • the inoculum for the pilot plant was prepared by taking 500 mL of the 3% synthetic medium culture and increasing the volume in several steps (including some spikes of perchlorate to high levels to increase biomass) until the culture was 20 gallons.
  • a spent brine solution from the ion-exchange process ion-exchange brine solution
  • ion-exchange brine solution was collected to be representative of an average of a fall range of brine solution quality encountered throughout a cycle of ion-exchange column regeneration.
  • the sample was transported in a headspace free 15-gallon container and stored at 4° C. until use in individual experiments. Chemical analysis and microbial characterization tests were conducted on the samples of brine as received. Table 2 lists the major cations present in the brine after dilution to 3% NaCl with deionized water.
  • the brine collected from the pilot plant for treatment was diluted to 3% NaCl by the addition of an equal amount of deionized water which had been boiled and cooled under a flush of nitrogen gas.
  • Ambient oxygen was purged from the brine by bubbling with oxygen-free nitrogen gas for approximately 1 hour and 0.3 mg/L resazurin was added as a redox indicator.
  • Inoculum from the 3% NaCl parent culture was prepared for use (i.e., the residual nutrient components from the parent culture were removed) by centrifuging the culture (1500 rpm, at 4° C.) for approximately 12-25 minutes. After centrifuging, the supernatant was decanted and resuspended in 3% NaCl solution. This procedure was repeated twice. The final harvested cell pellet was re-suspended in 3% NaCl solution and 2 mL of this suspension was added to about 100 mL of amended brine solution in a 150 mL serum bottle that had been flushed with N 2 gas for at least five minutes and then sealed with butyl rubber stoppers and aluminum crimp seals.
  • the results from Mg 2+ and Ca 2+ measurements showed that insignificant amounts of the cations were carried over with the inoculum.
  • the cultures were spiked with about 100 mg/L acetate and the appropriate amounts of concentrated metal ions (individually or all together) to adjust the concentrations of Mg 2+ to 130 mg/L, Ca 2+ to 40 mg/L, or K + to 40 mg/L as their chloride salts;
  • the initial pH of the brine was adjusted to 7.5 during the initial transfer and no pH adjustment was done during the subsequent SBR feeds.
  • the cultures were incubated while shaking at about 120 rpm at room temperature.
  • the performance of the resulting subcultures was compared with the performance of triplicate subcultures fed brine with no cation amendment.
  • the first SBR feed was accomplished by adding 60 mL of 3% diluted spent brine, and subsequent feeds were accomplished using true SBR procedures.
  • the cations and acetate were spiked directly into the cultures to the levels described above at the beginning of each feed cycle.
  • the magnesium and calcium concentrations were measured at the beginning and end of the experiment by flame atomic absorption spectrometry.
  • Liquid samples were taken using plastic sterile syringes and filtered through 0.20 ⁇ m syringe filter. The samples were kept in glass vials and refrigerated at 4° C. before analysis. Perchlorate concentrations were determined by using a Dionex DX-500 ion chromatograph (Dionex Corp., Sunnyvale, Calif.) equipped with a Dionex Ionpac AS164 mm separation column, an AG16 4 mm guard column, a GS50 gradient pump, an AS40 automated sampler, and a CD25 conductivity detector. An AMMS suppressor using 70 mM H 2 SO 4 solution as regenerant was also used in an external cycling mode. A 1000 ⁇ L sample loop was used to detect the low perchlorate concentrations in the ion-exchange brine. The eluent concentration was 65 mM KOH prepared with ultra-pure water with 18 M ⁇ cm resistivity.
  • Nitrate, acetate and sulfate analysis were performed using a Dionex DX-100 Ion chromatograph (Dionex Corp., Sunnyvale, Calif.) equipped with an IonPac AS12 4 mm separation column, an AG12 4 mm guard column, an AS40 automated sampler, an ASRS-ULTRA suppressor (100 mA), and a 25 ⁇ L sample loop.
  • the eluent used was a solution containing 0.3 mM NaHCO 3 and 2.7 mM Na 2 CO 3 and the flow rate was 1.25 mL/min.
  • Mg 2+ , Ca 2+ and K + concentrations were determined by flame flame atomic absorption spectrometry (Perkin Elmer, AAnalyst 300) equipped with Perkin Elmer LuminaTM Lamp. Volatile suspended solids (VSS) were measured according to the procedures described in Standard Methods (APHA, 1998).
  • Example results are presented in FIG. 2 , where a 60 g/L synthetic medium was tested to determine changes in microbial activity when each of the three above-identified ions are removed from the medium. As shown in FIG. 2 , the results showed that leaving out Mg 2+ , Ca 2+ , or K + caused a slowing of perchlorate degradation, i.e., removing each ion was detrimental to the operation of the culture to degrade perchlorate.
  • the inventors focused on the concentration of divalent cations and specifically on a mole ratio of divalent cations to monovalent cation (Na + ). Experiments were then directed to laboratory and pilot plant run to determine the effects of a divalent to monovalent cation mole ratio using M 2+ and/or Ca 2+ as the divalent cations. The experiments were directed to determine the divalent/monovalent cation mole ratio, as well as to determine which of these cations would allow the generation of brine solution that could support a stable culture and to determine the operating ranges of the brine solution.
  • Ca 2+ ions precipitated out of the brine due to high levels of carbonates we turned our attention to the addition of Mg 2+ ions, which did not precipitate in brine solution having high concentrations of carbonates ions.
  • the addition of either cation was beneficial: Ca 2+ briefly improved the perchlorate destruction rate in the brine solution prior to its elimination by precipitation, whereas Mg 2+ remained in the brine solution and improved its long-term performance for perchlorate destruction.
  • the inventors also found that the culture in brine solutions having a 60 g/L NaCl concentration required more Mg 2+ than the culture in brine solutions having a 30 g/L NaCl concentration, especially when nitrate is also present in the culture. These results verify that the requirement is not for a single concentration of divalent cations such as Mg 2+ , but for a ratio of divalent to monovalent cation mole ratio or the Mg 2+ to Na + mole ratio. Currently, the inventors know that when the ratio of divalent to monovalent cation mole ratio is at or above about 0.05 as shown in FIGS.
  • the cultures can reduce perchlorate rapidly in brine solution having 30 or 60 g/L NaCl, and when the ratio is increased, the culture performance increases as well.
  • This data evidenced that a minimum concentration of 600 mg/L of Mg 2+ in a brine solution including 30 g/L NaCl, which corresponds to a M 2+ /Na + mole ratio of at or above 0.05.
  • the inventors have developed a novel biological perchlorate destruction process for treating ion-exchange brine so that the brine solution can be reused or disposed of as non-hazardous waste.
  • This ion-exchange biological perchlorate destruction process eliminates perchlorate ion from waste brine solution and conserves regenerant brine solution for reuse.
  • the inventors have also discovered one preferred biologically stable brine solution for the destruction of perchlorate contaminated brine solutions, where the brine solution has sufficient magnesium ions to produce a magnesium to sodium or divalent to monovalent cation mole ratio ⁇ 0.05.
  • Ca 2+ ions can be added to the brine solution to adjust the divalent to monovalent cation mole ratio and achieve a biologically stable brine solution capable of microbial growth and proliferation, where the microbes are capable of decomposing, perchlorate.
  • Ca 2+ is not a preferred ion, because ion-exchange brines typically contain high concentrations of carbonates ion that tend to precipitate Ca 2+ ions.
  • using Ca 2+ ions as the divalent metal will require a Ca 2+ source be added to each batch or on a continuous basis, whereas Mg 2+ does not precipitate out, and is able to persist in the brine solution through the recycle process.
  • Ca 2+ or a mixture of Mg 2+ and Ca 2+ can be used in contaminated brine solutions having no or low concentrations of carbonates.
  • brine solutions contaminated with other non ion-exchangable pollutants can be treated in brine solutions having a divalent to monovalent mole ratio of at least 0.05.
  • the brine solution is adjusted to a divalent to monovalent cation mole ratio at or above about 0.05 and inoculated with microorganisms capable of growing in the stabilized brine solution and capable of anaerobic/anoxic degradation of the oil in the oil contaminated brine solution.
  • the brine solution is adjusted into the stable regime evidence by a divalent to monovalent cation mole ratio and inoculated with microorganisms capable of growing in the stabilized brine solution and capable of anaerobic/anoxic degradation of the pollutant in the pollutant contaminated brine solution.

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WO2012167002A1 (fr) * 2011-06-02 2012-12-06 General Electric Company Procédé et appareil de traitement du perchlorate dans approvisionnements en eau potable
CN104609504B (zh) * 2013-11-05 2016-08-17 中国科学院沈阳应用生态研究所 一种离子交换法转移并资源化回收并利用水中硝态氮的方法及装置
US10906827B2 (en) * 2016-10-24 2021-02-02 Koos Jan Baas Systems and methods for reducing algae blooms and microbial growth by phosphorus removal from aqueous systems
CN111675347A (zh) * 2020-05-25 2020-09-18 哈尔滨工业大学 一种完全混合式厌氧生物膜处理煤化工废水的方法
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